WO2015184816A1 - Nitrogen-doped graphene sheet and method for preparation and use thereof - Google Patents

Nitrogen-doped graphene sheet and method for preparation and use thereof Download PDF

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WO2015184816A1
WO2015184816A1 PCT/CN2015/071115 CN2015071115W WO2015184816A1 WO 2015184816 A1 WO2015184816 A1 WO 2015184816A1 CN 2015071115 W CN2015071115 W CN 2015071115W WO 2015184816 A1 WO2015184816 A1 WO 2015184816A1
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nitrogen
doped graphene
graphene sheet
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郑玉婴
汪晓莉
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福州大学
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

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  • the invention belongs to the field of preparation of supercapacitor electrode materials, and in particular relates to a nitrogen-doped graphene sheet and a preparation method and application thereof.
  • Traditional graphene nitrogen doping methods include chemical vapor deposition (CVD), plasma treatment, arc discharge, high-energy electrothermal, and templating.
  • CVD chemical vapor deposition
  • plasma treatment plasma treatment
  • arc discharge high-energy electrothermal
  • templating The preparation conditions are harsh and the doping amount is low (not higher than 8%). ), high production costs and other issues.
  • the doping method of the present invention can obtain high-quality and high-nitrogen nitrogen-doped graphene, and nitrogen-doped graphene can be prepared by changing the amount of nitrogen source.
  • the object of the present invention is to provide a nitrogen-doped graphene sheet, a preparation method and application thereof, no surfactant is used in the reaction process, the reactant composition is simple, the reaction condition is mild, and high-quality pure nitrogen-doped graphite is obtained.
  • An ene sheet, which has excellent electrochemical properties, can be used to prepare a supercapacitor electrode material.
  • the present invention adopts the following technical solutions:
  • Nitrogen-doped graphene sheets with high nitrogen content were prepared by a two-step process using ammonia as a nitrogen source. Includes the following steps:
  • the solvent is water or ethanol.
  • the nitrogen-doped graphene has a nitrogen content of greater than 8%.
  • the nitrogen-doped graphene sheets are used to prepare supercapacitor electrode materials.
  • the significant advantage of the invention is that the ammonia-doped graphene is prepared by a two-step method using ammonia as a nitrogen source, the experiment operation is simple, no dispersing agent is used, and the addition of ammonia water promotes the conversion of graphite oxide into graphene, and the obtained nitrogen blending.
  • the heterographene is a graphene sheet having a high nitrogen content and a large specific surface area.
  • Example 1 is an XRD chart of the undoped graphene sheets obtained in Example 1 and the nitrogen-doped graphene sheets obtained in Example 2.
  • Example 2 is a Raman diagram of nitrogen-doped graphene obtained in Example 2.
  • Example 3 is an SEM image of the nitrogen-doped graphene obtained in Example 2.
  • Example 4 is an XPS chart of nitrogen-doped graphene obtained in Example 1 and Example 2.
  • Fig. 5 is a charge and discharge diagram of the nitrogen-doped graphene obtained in Example 2.
  • Example 1 is an XRD chart of the undoped graphene sheets obtained in Example 1 and the nitrogen-doped graphene sheets obtained in Example 2. It can be seen from the figure that the reaction of oxidized graphite is reduced to graphene, and the nitrogen-doped graphene obtained by adding ammonia water is offset by 2 ⁇ angle, and the interlayer spacing is smaller, which is closer to the layer spacing of flake graphite, indicating that after doping The structure of the graphite was repaired.
  • 3 is an SEM image showing an 10,000-fold magnification of the nitrogen-doped graphene obtained in Example 2. From the figure, it can be seen that the nitrogen-doped graphene is a large graphene sheet.
  • FIG. 4 is an XPS diagram of nitrogen-doped graphene obtained in Example 1 and Example 2, which is clearly after doping The oxygen content is greatly reduced, the nitrogen content is significantly increased, and the prepared nitrogen-doped graphene has a nitrogen content of 11.75%, and the nitrogen content in the product can be adjusted by changing the amount of the nitrogen-containing compound.
  • Figure 5 is a charge and discharge diagram of nitrogen-doped graphene at 1 A/g with a specific capacitance of up to 110 F/g.

Abstract

Provided are a nitrogen-doped graphene sheet and a method for preparation and use thereof; taking aqueous ammonia as a nitrogen source, graphite oxide is added to a solvent and ultrasonically dispersed; next, concentrated aqueous ammonia is added and reacted at 40-150°C for 3-24 hours; then, a hydrothermal reaction is carried out at 80-200°C for 1-12 hours; after washing and drying, a nitrogen-doped graphene sheet is obtained. Also provided is a nitrogen-doped graphene sheet obtained using the method, and a use of the nitrogen-doped graphene sheet.

Description

一种氮掺杂石墨烯片及其制备方法和应用Nitrogen doped graphene sheet and preparation method and application thereof 技术领域Technical field
本发明属于超级电容器电极材料制备领域，具体涉及一种氮掺杂石墨烯片及其制备方法和应用。The invention belongs to the field of preparation of supercapacitor electrode materials, and in particular relates to a nitrogen-doped graphene sheet and a preparation method and application thereof.
背景技术Background technique
随着煤炭、石油、天然气等不可再生资源的不断枯竭以及环境污染的日益严重，研究和开发出新型环保的能量存储装置显得尤为迫切和重要。在此背景条件下，超级电容器应运而生，成为最有前途的能源存储设备之一。在大多数情况下，碳纳米材料如多孔碳材料，碳纳米管，石墨烯由于其大的表面积和高导电率，已被用来作为超级电容器的电极，但目前碳基材料仍处于发展阶段。石墨烯独特的原子结构和电子结构使得其表现出传统材料所不具有的多种非凡性能，超大的比表面积、可调节的带隙、高电子迁移率、优良的力学性能和光学性能等特点。目前，很多研究通过物理混合的方法制备石墨烯复合材料来提高其电化学性能，化学修饰的方法研究的比较少。其中最可行的化学修饰方法是通过掺杂，由于N原子具有与C原子近似的原子半径，可以作为电子供体对石墨烯进行掺杂，生成的氮掺杂石墨烯表现出较纯石墨烯更多优异的性能，拓宽了应用领域，包括生物传感器，燃料电池，以及电子器件的器件性能。With the continuous depletion of non-renewable resources such as coal, oil and natural gas and the increasing environmental pollution, it is particularly urgent and important to research and develop new environmentally friendly energy storage devices. Under this background, supercapacitors emerged as one of the most promising energy storage devices. In most cases, carbon nanomaterials such as porous carbon materials, carbon nanotubes, and graphene have been used as electrodes for supercapacitors due to their large surface area and high electrical conductivity, but carbon-based materials are still in the development stage. The unique atomic structure and electronic structure of graphene make it exhibit many extraordinary properties that traditional materials do not have, such as large specific surface area, adjustable band gap, high electron mobility, excellent mechanical properties and optical properties. At present, many studies have done to improve the electrochemical performance of graphene composites by physical mixing methods, and there are few studies on chemical modification methods. One of the most feasible chemical modification methods is by doping. Since the N atom has an atomic radius similar to that of the C atom, the graphene can be doped as an electron donor, and the resulting nitrogen-doped graphene exhibits a more pure graphene. The superior performance has broadened the application areas, including biosensors, fuel cells, and device performance of electronic devices.
传统的石墨烯氮掺杂的方法主要有化学气相沉积(CVD)法、等离子处理法、电弧放电法、高能电热法、模板法等，具有制备条件苛刻、掺杂量低(不高于8％)、生产成本高等问题。本发明的掺杂方法可以获得高品质和高含氮量的氮掺杂石墨烯，通过改变氮源的量可以调节制备不同掺杂量的氮掺杂石墨烯。Traditional graphene nitrogen doping methods include chemical vapor deposition (CVD), plasma treatment, arc discharge, high-energy electrothermal, and templating. The preparation conditions are harsh and the doping amount is low (not higher than 8%). ), high production costs and other issues. The doping method of the present invention can obtain high-quality and high-nitrogen nitrogen-doped graphene, and nitrogen-doped graphene can be prepared by changing the amount of nitrogen source.
发明内容Summary of the invention
本发明的目的在于提供一种氮掺杂石墨烯片及其制备方法和应用，反应过程中不使用任何表面活性剂，反应物成分简单，反应条件温和，制得高质量纯净的氮掺杂石墨烯片，其具有优异的电化学性能，可用于制备超级电容器电极材料。The object of the present invention is to provide a nitrogen-doped graphene sheet, a preparation method and application thereof, no surfactant is used in the reaction process, the reactant composition is simple, the reaction condition is mild, and high-quality pure nitrogen-doped graphite is obtained. An ene sheet, which has excellent electrochemical properties, can be used to prepare a supercapacitor electrode material.
为实现上述目的，本发明采用如下技术方案：To achieve the above object, the present invention adopts the following technical solutions:
以氨水作为氮源，通过两步法制得高含氮量的氮掺杂石墨烯片。包括以下步骤：Nitrogen-doped graphene sheets with high nitrogen content were prepared by a two-step process using ammonia as a nitrogen source. Includes the following steps:
(1)将氧化石墨加入到溶剂中超声分散，控制其浓度在1～10mg/mL；(1) adding graphite oxide to a solvent for ultrasonic dispersion, controlling the concentration thereof to be 1 to 10 mg / mL;
(2)加入浓氨水，浓氨水与氧化石墨的质量比为0.1～100；(2) adding concentrated ammonia water, the mass ratio of concentrated ammonia water to graphite oxide is 0.1-100;
(3)40～150℃反应3～24h； (3) 40 ~ 150 ° C reaction 3 ~ 24h;
(4)80～200℃水热反应1～12h；(4) hydrothermal reaction at 80 ~ 200 ° C for 1 ~ 12h;
(5)所得产物用去离子水冲洗数次，80℃下干燥12h，即得氮掺杂石墨烯片。(5) The obtained product was washed several times with deionized water and dried at 80 ° C for 12 h to obtain a nitrogen-doped graphene sheet.
所述的溶剂为水或乙醇。The solvent is water or ethanol.
所述的氮掺杂石墨烯的氮含量大于8％。The nitrogen-doped graphene has a nitrogen content of greater than 8%.
所述的氮掺杂石墨烯片用于制备超级电容器电极材料。The nitrogen-doped graphene sheets are used to prepare supercapacitor electrode materials.
本发明的显著优点在于：以氨水为氮源，采用两步法制备氮掺杂石墨烯，实验操作简单，不使用任何分散剂，氨水的加入促进了氧化石墨转化为石墨烯，得到的氮掺杂石墨烯为石墨烯片，含氮量高、比表面积大。The significant advantage of the invention is that the ammonia-doped graphene is prepared by a two-step method using ammonia as a nitrogen source, the experiment operation is simple, no dispersing agent is used, and the addition of ammonia water promotes the conversion of graphite oxide into graphene, and the obtained nitrogen blending. The heterographene is a graphene sheet having a high nitrogen content and a large specific surface area.
附图说明DRAWINGS
图1是实施例1所得的未掺杂石墨烯片和实施例2所得的氮掺杂石墨烯片的XRD图。1 is an XRD chart of the undoped graphene sheets obtained in Example 1 and the nitrogen-doped graphene sheets obtained in Example 2.
图2是实施例2所得氮掺杂石墨烯的拉曼图。2 is a Raman diagram of nitrogen-doped graphene obtained in Example 2.
图3是实施例2所得氮掺杂石墨烯的SEM图。3 is an SEM image of the nitrogen-doped graphene obtained in Example 2.
图4是实施例1和实施例2所得氮掺杂石墨烯的XPS图。4 is an XPS chart of nitrogen-doped graphene obtained in Example 1 and Example 2.
图5是实施例2所得氮掺杂石墨烯的充放电图。Fig. 5 is a charge and discharge diagram of the nitrogen-doped graphene obtained in Example 2.
具体实施方式detailed description
以下是本发明的几个具体实施例，进一步说明本发明，但是本发明不仅限于此。The invention is further illustrated by the following specific examples of the invention, but the invention is not limited thereto.
实施例1Example 1
首先将500mg经改进Hummers法制备的氧化石墨加入50mL的乙醇中，超声分散1h形成均匀的分散液后，在80℃的油浴锅中磁力搅拌反应10h，移至高压反应釜中，在150℃反应3h，所得产物用去离子水冲洗数次，然后在80℃下干燥12h，即得未掺杂产物。Firstly, 500 mg of graphite oxide prepared by the modified Hummers method was added to 50 mL of ethanol, and ultrasonically dispersed for 1 hour to form a uniform dispersion. After magnetic stirring in an oil bath at 80 ° C for 10 h, it was transferred to a high pressure reactor at 150 ° C. After 3 h of reaction, the obtained product was washed several times with deionized water and then dried at 80 ° C for 12 h to obtain an undoped product.
实施例2Example 2
首先将500mg经改进Hummers法制备的氧化石墨加入50mL的乙醇中，超声分散1h形成均匀的分散液后，加入2.5g浓氨水，然后在80℃的油浴锅中磁力搅拌10h，再移至高压反应釜中，在150℃反应3h，所得产物用去离子水冲洗数次，80℃下干燥12h，即得氮掺杂石墨烯片。所制备的氮掺杂石墨烯片的氮含量为11.75％。Firstly, 500 mg of graphite oxide prepared by the modified Hummers method was added to 50 mL of ethanol, and ultrasonically dispersed for 1 hour to form a uniform dispersion. Then, 2.5 g of concentrated ammonia water was added, and then magnetically stirred in an oil bath at 80 ° C for 10 hours, and then moved to a high pressure. In the reaction vessel, the reaction was carried out at 150 ° C for 3 h, and the obtained product was washed several times with deionized water and dried at 80 ° C for 12 h to obtain a nitrogen-doped graphene sheet. The prepared nitrogen-doped graphene sheets had a nitrogen content of 11.75%.
图1是实施例1所得的未掺杂石墨烯片和实施例2所得的氮掺杂石墨烯片的XRD图。从图中可以看出，经反应氧化石墨还原成石墨烯，加入氨水后得到的氮掺杂石墨烯2θ角发生偏移，层间距较小，更接近于鳞片石墨的层间距，说明掺杂后石墨的结构得到修复。图3是实施例2所得氮掺杂石墨烯的放大一万倍的SEM图，从图中可看出氮掺杂石墨烯为较大的石墨烯片状。图4是实施例1和实施例2所得氮掺杂石墨烯的XPS图，很明显掺杂之后 氧含量降低了很多，氮含量显著提高，所制备的氮掺杂石墨烯的氮含量为11.75％，通过改变含氮化合物的用量可以调节产品中的氮含量。图5是1A/g时氮掺杂石墨烯的充放电图，比电容高达110F/g。1 is an XRD chart of the undoped graphene sheets obtained in Example 1 and the nitrogen-doped graphene sheets obtained in Example 2. It can be seen from the figure that the reaction of oxidized graphite is reduced to graphene, and the nitrogen-doped graphene obtained by adding ammonia water is offset by 2θ angle, and the interlayer spacing is smaller, which is closer to the layer spacing of flake graphite, indicating that after doping The structure of the graphite was repaired. 3 is an SEM image showing an 10,000-fold magnification of the nitrogen-doped graphene obtained in Example 2. From the figure, it can be seen that the nitrogen-doped graphene is a large graphene sheet. 4 is an XPS diagram of nitrogen-doped graphene obtained in Example 1 and Example 2, which is clearly after doping The oxygen content is greatly reduced, the nitrogen content is significantly increased, and the prepared nitrogen-doped graphene has a nitrogen content of 11.75%, and the nitrogen content in the product can be adjusted by changing the amount of the nitrogen-containing compound. Figure 5 is a charge and discharge diagram of nitrogen-doped graphene at 1 A/g with a specific capacitance of up to 110 F/g.
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。 The above are only the preferred embodiments of the present invention, and all changes and modifications made to the scope of the present invention should fall within the scope of the present invention.

Claims (5)

  1. 一种氮掺杂石墨烯片的制备方法，其特征在于：以氨水作为氮源，通过两步法制得高含氮量的氮掺杂石墨烯片。A method for preparing a nitrogen-doped graphene sheet, characterized in that a nitrogen-containing graphene sheet having a high nitrogen content is obtained by a two-step method using ammonia water as a nitrogen source.
  2. 根据权利要求1所述的氮掺杂石墨烯片的制备方法，其特征在于：包括以下步骤：The method for preparing a nitrogen-doped graphene sheet according to claim 1, comprising the steps of:
    (1)将氧化石墨加入到溶剂中超声分散，控制其浓度在1～10mg/mL；(1) adding graphite oxide to a solvent for ultrasonic dispersion, controlling the concentration thereof to be 1 to 10 mg / mL;
    (2)加入浓氨水，浓氨水与氧化石墨的质量比为0.1～100；(2) adding concentrated ammonia water, the mass ratio of concentrated ammonia water to graphite oxide is 0.1-100;
    (3)40～150℃反应3～24h；(3) 40 ~ 150 ° C reaction 3 ~ 24h;
    (4)80～200℃水热反应1～12h；(4) hydrothermal reaction at 80 ~ 200 ° C for 1 ~ 12h;
    (5)所得产物用去离子水冲洗数次，80℃下干燥12h，即得氮掺杂石墨烯片。(5) The obtained product was washed several times with deionized water and dried at 80 ° C for 12 h to obtain a nitrogen-doped graphene sheet.
  3. 根据权利要求2所述的氮掺杂石墨烯片的制备方法，其特征在于：所述的溶剂为水或乙醇。The method according to claim 2, wherein the solvent is water or ethanol.
  4. 一种如权利要求1所述的方法制得的氮掺杂石墨烯片，其特征在于：所述的氮掺杂石墨烯的氮含量大于8％。A nitrogen-doped graphene sheet produced by the method of claim 1, wherein the nitrogen-doped graphene has a nitrogen content of greater than 8%.
  5. 一种如权利要求1所述的方法制得的氮掺杂石墨烯片的应用，其特征在于：所述的氮掺杂石墨烯片用于制备超级电容器电极材料。 Use of a nitrogen-doped graphene sheet produced by the method of claim 1 wherein said nitrogen-doped graphene sheet is used to prepare a supercapacitor electrode material.
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